US12423964B2 - Intelligent system for determining hemp by headspace chemical analysis - Google Patents
Intelligent system for determining hemp by headspace chemical analysisInfo
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- US12423964B2 US12423964B2 US17/706,524 US202217706524A US12423964B2 US 12423964 B2 US12423964 B2 US 12423964B2 US 202217706524 A US202217706524 A US 202217706524A US 12423964 B2 US12423964 B2 US 12423964B2
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- G—PHYSICS
- G06—COMPUTING OR CALCULATING; COUNTING
- G06V—IMAGE OR VIDEO RECOGNITION OR UNDERSTANDING
- G06V10/00—Arrangements for image or video recognition or understanding
- G06V10/70—Arrangements for image or video recognition or understanding using pattern recognition or machine learning
- G06V10/82—Arrangements for image or video recognition or understanding using pattern recognition or machine learning using neural networks
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- G—PHYSICS
- G06—COMPUTING OR CALCULATING; COUNTING
- G06V—IMAGE OR VIDEO RECOGNITION OR UNDERSTANDING
- G06V10/00—Arrangements for image or video recognition or understanding
- G06V10/40—Extraction of image or video features
- G06V10/44—Local feature extraction by analysis of parts of the pattern, e.g. by detecting edges, contours, loops, corners, strokes or intersections; Connectivity analysis, e.g. of connected components
- G06V10/443—Local feature extraction by analysis of parts of the pattern, e.g. by detecting edges, contours, loops, corners, strokes or intersections; Connectivity analysis, e.g. of connected components by matching or filtering
- G06V10/449—Biologically inspired filters, e.g. difference of Gaussians [DoG] or Gabor filters
- G06V10/451—Biologically inspired filters, e.g. difference of Gaussians [DoG] or Gabor filters with interaction between the filter responses, e.g. cortical complex cells
- G06V10/454—Integrating the filters into a hierarchical structure, e.g. convolutional neural networks [CNN]
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- G—PHYSICS
- G06—COMPUTING OR CALCULATING; COUNTING
- G06V—IMAGE OR VIDEO RECOGNITION OR UNDERSTANDING
- G06V10/00—Arrangements for image or video recognition or understanding
- G06V10/70—Arrangements for image or video recognition or understanding using pattern recognition or machine learning
- G06V10/77—Processing image or video features in feature spaces; using data integration or data reduction, e.g. principal component analysis [PCA] or independent component analysis [ICA] or self-organising maps [SOM]; Blind source separation
- G06V10/774—Generating sets of training patterns; Bootstrap methods, e.g. bagging or boosting
Definitions
- hemp is defined as cannabis with less than 0.3% THC (tetrahydrocannabinol). Cannabis containing more than 0.3% THC is still a Schedule 1 controlled substance under federal law. Thus, determining the THC content of cannabis is useful for differentiating between ordinary agricultural commodities and controlled substances.
- THC tetrahydrocannabinol
- Typical methods for determining the THC content of cannabis include liquid extraction of THC from a cannabis sample using solvents. Therefore, there is a need for non-destructive, non-solvent based methods for determining THC content in cannabis samples.
- FIG. 1 depicts examples of images generated from GC/MS data for a placebo marijuana sample and a marijuana sample.
- FIG. 2 depicts an example workflow for generating images from GC/MS data and using the images in a deep learning neural network.
- FIG. 3 depicts an example of a plot of accuracy versus loss per epoch.
- FIG. 4 depicts an example comparison of conventional laboratory testing workflow (“Workflow 1”) and proposed AI workflow (“Workflow 2”) for headspace-GC/MS analysis of hemp and marijuana determination using the embodiments described herein.
- FIG. 5 depicts results of preliminary testing of four random hemp control samples.
- FIG. 6 depicts a preliminary result for the identification of THC and other cannabinoids from 250 ⁇ L of headspace gas samples.
- FIG. 7 is a flow diagram illustrating a method for assessing a cannabis sample, according to some embodiments
- FIG. 8 is a block diagram of one embodiment of a computer system.
- the term “based on” is used to describe one or more factors that affect a determination. This term does not foreclose the possibility that additional factors may affect the determination. That is, a determination may be solely based on specified factors or based on the specified factors as well as other, unspecified factors.
- a determination may be solely based on specified factors or based on the specified factors as well as other, unspecified factors.
- the phrase “in response to” describes one or more factors that trigger an effect. This phrase does not foreclose the possibility that additional factors may affect or otherwise trigger the effect. That is, an effect may be solely in response to those factors, or may be in response to the specified factors as well as other, unspecified factors.
- the terms “first,” “second,” etc. are used as labels for nouns that they precede, and do not imply any type of ordering (e.g., spatial, temporal, logical, etc.), unless stated otherwise.
- the term “or” is used as an inclusive or and not as an exclusive or.
- the phrase “at least one of x, y, or z” means any one of x, y, and z, as well as any combination thereof (e.g., x and y, but not z).
- the context of use of the term “or” may show that it is being used in an exclusive sense, e.g., where “select one of x, y, or z” means that only one of x, y, and z are selected in that example.
- Embodiments disclosed herein present a system and method for determining the THC content of cannabis samples.
- Specific embodiments implement machine learning algorithms (e.g., convolutional neural networks) to determine whether the THC content of a cannabis sample is above or below a predetermined threshold.
- the predetermined threshold is a threshold that differentiates between hemp and non-hemp cannabis.
- the concentration levels of THC (tetrahydrocannabinol) and CBD (cannabidiol) in cannabis plant materials typically range from below 0.1% to 10%, or even higher.
- the present disclosure recognizes that a sufficient amount of THC and CBD can be rapidly detected from a sample headspace without the use of additional adsorption traps, such as SPME (solid-phase microextraction) fibers or Tenax sorbent tubes.
- a headspace-GC/MS gas chromatography/mass spectrometer
- hemp determination workflow may be developed in a forensic laboratory where a GC/MS is commonly equipped.
- ground-truth samples e.g., hemp plant materials with known levels of THC and CBD
- a machine learning model e.g., convolutional neural network (CNN)
- AI artificial intelligence
- performance of AI in determining hemp samples may be evaluated by a random selection of known hemp and non-hemp samples. False-positive and false-negative rates of the new approach may also be determined to refine AI performance.
- the sample size, headspace vial size, sampling temperature, and sampling volume of GC/MS may be optimized to improve the analytical performance of headspace-GC/MS for hemp plant materials.
- a rapid headspace sampling procedure may utilize a thermostat to heat the sample vials before sampling headspace for GC/MS by using an air-tight syringe.
- standard hemp samples are analyzed by both HPLC (high-pressure liquid chromatography) and headspace-GC/MS for comparison.
- HPLC high-pressure liquid chromatography
- headspace-GC/MS headspace-GC/MS
- THC levels might increase due to decarboxylation of THCA (tetrahydrocannabinolic acid) or isomerization of CBD
- the HPLC test may be implemented for common cannabinoids without issues related to heating the sample. It is believed that a rapid heated-headspace sampling procedure should not alter the levels of THC in the samples. Comparing testing using the HPLC dataset and headspace-GC/MS dataset from the same variety of hemp samples may be used to verify that the rapid heated-headspace sampling procedure does not alter the levels of THC. Ground-truth hemp datasets may be used for these comparisons.
- a headspace-GC/MS dataset may be processed by both a traditional approach and the AI (CNN) approach.
- the traditional approach includes a calibration method using peak areas of THC in the total ion chromatograms (TIC) or extracted ion chromatograms (EIC) using phenanthrene or stable isotope-labeled THC as an internal standard.
- the calibration method that produces a better calibration range for THC may be implemented for comparison to the AI (CNN) approach.
- deuterated-THC may be used as an internal standard for quantitative analysis of THC. The use of deuterated-THC may, however, be less preferable as its use increases the cost for each test and the test of hemp and marijuana is not a trace chemical analysis.
- the use of phenanthrene as an internal standard may be sufficient to quantify THC at milligram levels.
- the calculated THC percentage measured by headspace-GC/MS can be compared to the HPLC method to determine the accuracy and precision of headspace-GC/MS.
- AI artificial intelligence
- measurement data from a headspace sampling by GC/MS is transformed into one or more images for assessment by an AI system (e.g., a CNN).
- headspace GC/MS data e.g., GC/MS signals
- Matlab or another commercially available program with a deep learning toolbox may be implemented for the transformation of headspace GC/MS data into images.
- headspace GC/MS data is transformed based on retention time, mass scan range, and signal intensity in the data.
- retention time, scan range, and signal intensities may be extracted from the headspace GC/MS data and these features may be used to generate the one or more images.
- the signal intensity is normalized using an internal standard before generating the one or more images.
- FIG. 1 depicts examples of images generated from GC/MS data for a placebo marijuana sample and a marijuana sample. Images, such as those depicted in FIG. 1 , may be assessed using an AI model such as a CNN to determine chemical information for the GC/MS data without using a conventional GC/MS data analysis approach that determines chemical information for each peak in the GC/MS data. In certain embodiments, CNN assessment of such images may determine whether a cannabis sample is a hemp sample or a marijuana (non-hemp) sample.
- an AI model such as a CNN to determine chemical information for the GC/MS data without using a conventional GC/MS data analysis approach that determines chemical information for each peak in the GC/MS data.
- CNN assessment of such images may determine whether a cannabis sample is a hemp sample or a marijuana (non-hemp) sample.
- a deep learning model such as CNN is trained to recognize chemical features representing hemp and non-hemp images as constructed from their headspace-GC/MS data.
- the CNN may be trained to recognize THC content in reference images generated from GC/MS data of cannabis samples.
- the reference images include images generated from ground-truth hemp data.
- the CNN may be trained to recognize chemical features in the reference images to determine whether a sample is hemp or non-hemp.
- a CNN is trained to assess one or more images generated from GC/MS data for a cannabis sample and determine whether the cannabis sample is hemp or non-hemp (e.g., non-marijuana or marijuana). For example, the CNN may be trained to determine whether the THC content is above or below a predetermined threshold (e.g., above or below 0.3% THC) based on the images themselves, which may be a threshold differentiating between hemp and non-hemp.
- a predetermined threshold e.g., above or below 0.3% THC
- Using CNN to determine whether a cannabis sample is hemp or non-hemp can be implemented in a variety of environments. For instance, CNN analysis may be implemented in forensic laboratory applications and/or field-deployable platforms.
- headspace data obtained by headspace-GC/MS may be processed using the following steps:
- FIG. 2 depicts an example workflow for generation of images from GC/MS data and using the images in a deep learning neural network.
- GC/MS analysis is performed on dried cannabis plant 210 .
- the GC/MS analysis data may include a transform of the chemical data into image data, represented by heat map 220 .
- Heat map 220 may then be input and transformed through a CNN.
- a visualization of the CNN architecture is illustrated in 230 .
- a build of a convolutional neural network involves three convolutions operating on 3 ⁇ 3 windows, an ReLU (rectified linear unit), and max-pooling modules operating on 2 ⁇ 2 windows.
- the first convolution may extract 16 filters, the following one may extract 32 filters, and the last convolution may extract 64 filters.
- two fully connected layers may be programmed, ending the network with sigmoid activation.
- two data generators one for training and one for validation may be setup.
- images are normalized for processing by the CNN using normalized pixel values.
- the CNN is trained for 15 epochs and validated. The performance of the CNN may be visualized, for example, by plotting the accuracy and loss per epoch.
- FIG. 3 depicts an example of a plot of accuracy versus loss per epoch.
- accuracy is defined as being the sum of (true positives and true negatives) divided by the sum of (true positives and false positives and true negatives and false negatives).
- AI CNN
- FIG. 3 shows that after 15 epochs of training for the CNN (AI) model, an embodiment of the algorithm can successfully determine hemp with more than 99% accuracy.
- the blue trace is training accuracy
- the orange trace is validation accuracy.
- training accuracy and validation accuracy are both above 95%.
- the accuracy and validation metrics demonstrate that transformation of GC/MS data into images is implementable for a developed deep learning process to generate AI that may accurately assess cannabis samples.
- the trained AI model can provide accurate categorical decisions of hemp/non-hemp without the use of a cut-off value of 0.3% THC for hemp determination (as the AI model may determine hemp/non-hemp based on the images themselves without any calculated determination of the THC content).
- the chemical signatures captured by headspace chemical analysis have excellent potential for hemp determination.
- headspace chemical analysis may capture chemical signatures for a differentiation between true marijuana (marijuana with THC and CBD) and placebo marijuana (marijuana samples with THC less than 0.01% and no CBD).
- the AI model e.g., CNN
- the accuracy of the AI model may also be verified with the ground-truth hemp samples and, in some embodiments, the precision of the model can be improved with a larger size training dataset.
- the headspace-GC/MS analytical testing platform described herein may be combined with new data sciences to offer a novel method for the statistical interpretation of evidence. Moreover, the entire testing process from chemical analysis to data processing may be automated and standardized.
- FIG. 4 depicts an example comparison of conventional laboratory testing workflow (“Workflow 1”) and proposed AI workflow (“Workflow 2”) for headspace-GC/MS analysis of hemp and marijuana determination using the embodiments described herein.
- workflow 400 implements either workflow 1 405 A (e.g., the conventional workflow) or workflow 2 405 B (e.g., the AI/CNN workflow).
- Workflow 400 begins with collecting a sample in sampling in 410 . The sample is then provided to headspace GC/MS Analysis tool 420 . Tool 420 then generates headspace GC/MS data 430 . Data 430 may be in a typical chromatogram format as shown above data 430 .
- conventional data analysis is conducted on data 430 in 440 .
- Conventional data analysis 440 may include, for example, analysis of the signal versus concentration to determine THC concentration values in the sample. These THC concentration values may be compared to a THC threshold in 450 to determine whether the THC concentration in the sample is above or below the THC threshold (e.g., a THC cut-off value). This threshold comparison may determine whether the sample has a particular value of THC indicating cannabis (e.g., whether sample is hemp or non-hemp).
- image data analysis 470 includes implementation of a convolutional neural network (CNN), as described herein.
- CNN image data analysis 470 may output, for example, a classification as to whether the sample is hemp or non-hemp.
- accuracy of CNN image data analysis 470 may be determined based on a ROC curve and confusion matrix such as shown in 490 .
- FIG. 5 depicts results of preliminary testing of the four random hemp control samples. Approximately 40 mg hemp samples were placed in a 10 mL headspace vial. After heating the sample in the vial to 150° C. for 5 minutes, 250 ⁇ L headspace gas was sampled by an air-tight syringe for GC/MS analysis. As shown in FIG. 5 , a general GC oven program heating from 50° C. to 300° C. could readily separate headspace chemicals within 15 minutes. The headspace sampling was capable of rapidly transferring cannabinoids for GC/MS analysis, as well as terpenes and chlorophyll from the plant materials.
- headspace chemical analysis produces representative chemical features for the qualitative and quantitative chemical analysis of cannabinoids for marijuana plant materials.
- direct headspace sampling provides the same degree of confidence for the determination of hemp and marijuana samples in a shorter amount of time than other typical analysis techniques.
- FIG. 6 depicts a preliminary result for the identification of THC and other cannabinoids from 250 ⁇ L of headspace gas samples.
- the GC oven was initially set at 150° C., then increased to 300° C. with a ramp of 25° C./min.
- a sufficient resolution for THC and other cannabinoids may be reached with shortened GC/MS runtimes (e.g., less than 5 minutes).
- the chromatogram in FIG. 6 depicts the potential for the headspace-GC/MS approach. Additionally, preliminary data also demonstrates that cleaner headspace sampling of the cannabinoid from hemp samples may be achieved for the GC/MS testing workflow (e.g., “Workflow 2”), shown in FIG. 4 .
- FIG. 7 is a flow diagram illustrating a method for assessing a cannabis sample, according to some embodiments.
- the method shown in FIG. 7 may be used in conjunction with any of the computer circuitry, systems, devices, elements, or components disclosed herein, among other devices.
- some of the method elements shown may be performed concurrently, in a different order than shown, or may be omitted. Additional method elements may also be performed as desired.
- some or all elements of this method may be performed by a particular computer system, such as computing device 810 , described below.
- a computer system accesses a set of data for a cannabis sample where the set of data includes data acquired from gas chromatography/mass spectrometer measurements of a headspace of the cannabis sample.
- the computer system transforms the set of data into one or more images based on retention time, scan range, and signal intensities in the set of data.
- the computer system assesses the one or more images using a convolutional neural network to determine whether the cannabis sample is hemp or non-hemp.
- computing device 810 may be used to implement various portions of this disclosure.
- Computing device 810 may be any suitable type of device, including, but not limited to, a personal computer system, desktop computer, laptop or notebook computer, mainframe computer system, web server, workstation, or network computer.
- computing device 810 includes processing unit 850 , storage 812 , and input/output (I/O) interface 830 coupled via an interconnect 860 (e.g., a system bus).
- I/O interface 830 may be coupled to one or more I/O devices 840 .
- Computing device 810 further includes network interface 832 , which may be coupled to network 820 for communications with, for example, other computing devices.
- processing unit 850 includes one or more processors. In some embodiments, processing unit 850 includes one or more coprocessor units. In some embodiments, multiple instances of processing unit 850 may be coupled to interconnect 860 . Processing unit 850 (or each processor within 850 ) may contain a cache or other form of on-board memory. In some embodiments, processing unit 850 may be implemented as a general-purpose processing unit, and in other embodiments it may be implemented as a special purpose processing unit (e.g., an ASIC). In general, computing device 810 is not limited to any particular type of processing unit or processor subsystem.
- module refers to circuitry configured to perform specified operations or to physical non-transitory computer readable media that store information (e.g., program instructions) that instructs other circuitry (e.g., a processor) to perform specified operations.
- Modules may be implemented in multiple ways, including as a hardwired circuit or as a memory having program instructions stored therein that are executable by one or more processors to perform the operations.
- a hardware circuit may include, for example, custom very-large-scale integration (VLSI) circuits or gate arrays, off-the-shelf semiconductors such as logic chips, transistors, or other discrete components.
- VLSI very-large-scale integration
- a module may also be implemented in programmable hardware devices such as field programmable gate arrays, programmable array logic, programmable logic devices, or the like.
- a module may also be any suitable form of non-transitory computer readable media storing program instructions executable to perform specified operations.
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Abstract
Description
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- 1. Data export: GC/MS data may be saved in a .CDF format, which can be processed in a Matlab environment.
- 2. Transform GC/MS data into images: As described above, retention time, scan range, and signal intensities in the GC/MS data may be extracted to generate images for each cannabis sample. Signal intensity may be normalized by an internal standard before generating the images.
- 3. Intelligent data analysis using deep learning: A deep learning neural network, using a CNN, may be implemented for feature extraction and pattern analysis of the generated images to determine hemp/non-hemp properties of the cannabis samples. In certain embodiments, ground-truth hemp data is used for training the deep learning neural network.
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